CN110806369A - Method for detecting performance of dispersing agent - Google Patents
Method for detecting performance of dispersing agent Download PDFInfo
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- CN110806369A CN110806369A CN201810886821.8A CN201810886821A CN110806369A CN 110806369 A CN110806369 A CN 110806369A CN 201810886821 A CN201810886821 A CN 201810886821A CN 110806369 A CN110806369 A CN 110806369A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The application provides a method for detecting the performance of a dispersant. The detection method comprises the following steps: step S1, adding a dispersant solution and a polymer to be polymerized into a container to obtain a mixture; step S2, heating the container to heat the mixture to a preset temperature and keep the temperature for a preset time to obtain a product; and step S3, measuring the particle size of the product, and judging the performance of the dispersing agent according to the particle size. According to the detection method, the dispersing agent and the polymer to be polymerized are added into the container, and then the heated container enables the polymer to be polymerized to react, so that the real situation in the recovery tower is simulated.
Description
Technical Field
The application relates to the field of dispersant detection, in particular to a method for detecting the performance of a dispersant.
Background
Acrylonitrile, hydrocyanic acid and acrolein in the recovery tower of the acrylonitrile device are easy to polymerize, and the produced polymer is attached to the tower plate of the recovery tower to form blocky organic scale, so that the tower plate is blocked, and the device needs to be stopped.
To solve the above technical problem, a small amount of dispersant is usually added to the feed line of the recovery column to prevent the polymer from forming lumpy organic scale on the trays. In the research and development of a dispersant formula, in order to determine whether the selected dispersant can meet the application effect, an evaluation experiment needs to be carried out to evaluate the scale inhibitor.
Publication No. CN200980146776 describes a laboratory evaluation method, which comprises adding a dispersant solution into rich water to prepare the rich water with a target concentration, adding the rich water and polymer powder into a glass test tube, and observing whether a precipitate exists at the bottom of the test tube after sufficient shock. The method only evaluates the organic scale which is agglomerated, is inconsistent with the practical application environment of the dispersant in the recovery tower, cannot accurately reflect the application effect of the dispersant, and cannot quantitatively evaluate the application effect of the dispersant.
The above information disclosed in this background section is only for enhancement of understanding of the background of the technology described herein and, therefore, certain information may be included in the background that does not form the prior art that is already known in this country to a person of ordinary skill in the art.
Disclosure of Invention
The main purpose of the present application is to provide a method for detecting the performance of a dispersant, so as to solve the problem that the method for detecting the performance of a dispersant in the prior art cannot accurately detect the performance of a dispersant.
In order to achieve the above object, according to one aspect of the present application, there is provided a method of detecting performance of a dispersant, the method comprising: step S1, adding a dispersant solution and a polymer to be polymerized into a container to obtain a mixture; step S2, heating the container to heat the mixture to a preset temperature and keep the temperature for a preset time to obtain a product; and step S3, measuring the particle size of the product, and judging the performance of the dispersant according to the particle size.
Further, in the dispersant solution, the mass percent of the dispersant is 10-55%, preferably, the volume of the dispersant solution is 0.03-0.5% of the volume of the container, and the volume of the polymer to be polymerized is 1/150-1/20% of the volume of the container.
Further, in step S1, an initiator is further added to the container, and the mixture further includes an initiator, and preferably, the volume of the initiator is 0.38 to 6.15% of the volume of the container.
Further, the initiator is a composite initiator, preferably the polymer is acrylonitrile, and the composite initiator comprises concentrated sulfuric acid, a potassium persulfate solution and a sodium thiosulfate solution.
Further, in the concentrated sulfuric acid, the mass percent of sulfuric acid is 95-99%; in the potassium persulfate solution, the mass percent of the potassium persulfate solution is between 1 and 4 percent; in the sodium thiosulfate solution, the mass percent of the sodium thiosulfate is between 1 and 20 percent.
Further, the volume of the concentrated sulfuric acid is 0.02 to 0.15% of the volume of the container, the volume of the potassium persulfate solution is 0.33 to 5% of the volume of the container, and the volume of the sodium thiosulfate solution is 0.03 to 1% of the volume of the container.
Further, in the step S1, a solvent is further added to the container, and the mixture further includes the solvent, and preferably, the volume of the solvent is 1/3 to 1/2 of the volume of the container.
Further, after the step S1, the detecting method further includes: the mixture was stirred.
Further, the stirring speed is between 200r/min and 240 r/min.
Further, the mixture is stirred by a stirring device, and the stirring device comprises a stirring rod, a speed regulator and a motor.
Further, the detection method further comprises: condensing the gaseous polymer to be polymerized in the container, so that the gaseous polymer to be polymerized is converted into the liquid polymer to be polymerized.
Further, the above-mentioned polymer to be polymerized in a gaseous state is condensed by a condenser, and it is preferable that the above-mentioned condenser is a condensation tube.
Further, the predetermined temperature is 50-90 ℃, and the predetermined time is 6-8 h.
Further, in step S2, the container is heated in a constant temperature water bath.
Further, the container is a three-neck flask, and the three-neck flask is placed in the constant temperature water bath.
Further, in the above step S3, by measuring the particle size of the product.
By applying the technical scheme, the dispersing agent and the polymer to be polymerized are added into the container in the detection method, and then the container is heated to enable the polymer to be polymerized to react, so that the real situation in the recovery tower is simulated.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the application and, together with the description, serve to explain the application and are not intended to limit the application. In the drawings:
FIG. 1 shows a schematic flow diagram of a detection method in an embodiment according to the present application; and
fig. 2 shows a schematic structural diagram of an apparatus for implementing the detection method in an embodiment according to the present application.
Wherein the figures include the following reference numerals:
10. a stand; 20. a thermometer; 30. a container; 40. a motor; 50. a speed regulator; 60. a condenser; 70. a constant temperature water bath; 80. a low temperature water bath; 90. a stirring rod.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
It will be understood that when an element such as a layer, film, region, or substrate is referred to as being "on" another element, it can be directly on the other element or intervening elements may also be present. Also, in the specification and claims, when an element is described as being "connected" to another element, the element may be "directly connected" to the other element or "connected" to the other element through a third element.
As described in the background art, the method for detecting the performance of the dispersant in the prior art cannot accurately detect the performance of the dispersant, and in order to solve the above problem, the present application proposes a method for detecting the performance of the dispersant.
In an exemplary embodiment of the present application, a method for testing the performance of a dispersant is provided, as shown in fig. 1, the method comprising: step S1, adding a dispersant solution and a polymer to be polymerized into a container to obtain a mixture; step S2, heating the container to heat the mixture to a preset temperature and keep the temperature for a preset time to obtain a product; and step S3, measuring the particle size of the product, and judging the performance of the dispersant according to the particle size. When different dispersants are detected, when the test conditions are consistent, the smaller the particle size of the product is, the better the dispersing effect of the dispersant is. Conversely, the larger the particle size of the product, the poorer the dispersing effect of the dispersant.
In the detection method, the dispersant and the polymer to be polymerized are added into the container, and then the container is heated to enable the polymer to be polymerized to react, so that the real situation in the recovery tower is simulated.
In an embodiment of the present application, in the dispersant solution, a mass percentage of the dispersant is between 10% and 55%. Therefore, the dispersing agent can be completely dissolved in the solvent, and the evaluation result is more accurate. The solution was none.
In a specific embodiment, the volume of the dispersant solution is 0.03-0.5% of the volume of the container, and the volume of the polymer to be polymerized is 1/150-1/20% of the volume of the container. This allows a further better simulation of the concentration of polymer to be obtained on the partial trays of the recovery column, while allowing the dispersant to disperse the polymer formed by the polymerization reaction in the solvent.
In order to improve the detection efficiency and ensure the accuracy of the detection result, in an embodiment of the present application, in step S1, an initiator is further added to the container, and the mixture further includes an initiator.
In another embodiment of the present application, the volume of the initiator is 0.38 to 6.15% of the volume of the container. Therefore, the detection efficiency and the detection accuracy can be better considered.
The initiator used in the present application may be any material that can initiate polymerization of the polymer, and those skilled in the art can select a suitable material as the initiator according to the actual situation, for example, the specific material of the initiator is determined according to the kind of the polymer to be polymerized.
In order to better initiate the polymerization of the polymer to be polymerized and at the same time to further ensure the accuracy of the detection method, the initiator is a composite initiator.
In a specific embodiment of the present application, the polymer is acrylonitrile, and the composite initiator includes concentrated sulfuric acid, a potassium persulfate solution, and a sodium thiosulfate solution.
In order to further ensure the detection efficiency of the detection method and the detection accuracy of the detection method, in an embodiment of the application, the mass percentage of sulfuric acid in the concentrated sulfuric acid is 95-99%; in the potassium persulfate solution, the mass percent of the potassium persulfate solution is between 1 and 4 percent; in the sodium thiosulfate solution, the mass percent of the sodium thiosulfate is between 1 and 20 percent.
In still another embodiment of the present invention, the volume of the concentrated sulfuric acid is 0.02 to 0.15% of the volume of the container, the volume of the potassium persulfate solution is 0.33 to 5% of the volume of the container, and the volume of the sodium thiosulfate solution is 0.03 to 1% of the volume of the container. Therefore, the detection efficiency of the detection method can be further ensured, and the detection accuracy of the detection method can be ensured at the same time.
In order to more truly simulate the real environment in which the polymer is to be present, and thus to more accurately determine the performance of the dispersant, in one embodiment of the present application, a solvent is also added to the container in step S1, and the mixture further includes the solvent.
And in order to further truly simulate the real environment in which the polymer exists, the volume of the solvent is 1/2-1/3 of the volume of the container.
In another embodiment of the present application, after step S1, the detecting method further includes: the mixture is stirred, so that the mixture can be mixed more uniformly, the environment where the polymer exists can be simulated more truly, and the performance of the dispersing agent can be judged more accurately.
In order to improve the mixing effect of the solvent, the polymer to be polymerized, the composite initiator and the dispersant, in one embodiment of the present application, the stirring speed is between 200r/min and 240 r/min.
In a specific embodiment, the stirring process is performed by a stirring device, as shown in fig. 2, which includes a stirring rod 90, a speed governor 50, and a motor 40.
Of course, the stirring device in the present application is not limited to the above structure, and other stirring devices in the prior art may be used, and those skilled in the art may select a device with a suitable structure to stir according to actual situations.
In order to change a part of the polymer to be polymerized into a gas state after heating the container, and to prevent the polymer to be polymerized from diffusing out of the container to affect the determination of the performance of the dispersant, the detection method further includes: condensing the gaseous polymer to be polymerized in the container, so that the gaseous polymer to be polymerized is converted into the liquid polymer to be polymerized.
The above-mentioned condensation process of the present application can be implemented by any feasible device in the prior art, and those skilled in the art can select a suitable device to perform the condensation process according to actual situations. In one embodiment of the present application, a condenser 60 is used to condense the above-mentioned polymer to be polymerized in a gaseous state, as shown in FIG. 2.
In order to perform condensation in a simpler manner, in one embodiment of the present application, the condenser 60 is a condenser tube, as shown in fig. 2.
In still another embodiment of the present application, the predetermined temperature is between 50 ℃ and 90 ℃, and the predetermined time is between 6h and 8h, so that the environment in which the polymer is to be present can be further simulated truly, the performance of the dispersant can be determined more accurately, and the detection efficiency can be further improved.
In a specific implementation, in step S2, the container 30 is heated in the constant temperature water bath 70 as shown in fig. 2. This makes it easier to heat the container 30.
In a specific embodiment, as shown in FIG. 2, the container 30 is a three-necked flask, and the three-necked flask is placed in the constant temperature water bath 70. As shown in fig. 2, the three-necked flask is a flask having three openings, one opening for inserting a stirring rod 90, the other opening for inserting a thermometer 20, the thermometer 20 for measuring the temperature of the mixture in the container 30, and the other opening for inserting a condenser 60.
Of course, the container 30 in the present application is not limited to the three-necked flask described above, and may be a container 30 having another structure.
In one embodiment of the present application, the acrylonitrile is an industrial product containing no polymerization inhibitor and having a mass fraction of 99% or more.
In order to make the technical solutions of the present application more clearly understood by those skilled in the art, the technical solutions and technical effects of the present application will be described below with reference to specific embodiments.
In a specific example, the container used in the examples of the present application is a 500mL three-neck flask, but is not limited to a 500mL three-neck flask, and the structure and volume of the container can be adjusted by one skilled in the art according to the circumstances.
Example 1
The detection apparatus shown in fig. 2 is used to carry out a specific detection process, and the detection apparatus shown in fig. 2 includes a stand 10, a thermometer 20, a container 30, a motor 40, a speed controller 50, a condenser 60, a constant temperature water bath 70, a low temperature water bath 80, and a stirring rod 90, wherein the container is a three-necked flask, one opening is used for inserting the stirring rod 90, the other opening is used for inserting the thermometer 20, the thermometer is used for measuring the temperature of a mixture in the container, the other opening is used for inserting the condenser 60, the container 30 is placed in the constant temperature water bath 70, the condenser 60 is communicated with the low temperature water bath 80, the low temperature water bath 80 is used for supplying cold water to the condenser, and the condenser is a condenser tube in.
The specific detection process comprises the following steps:
in the detection apparatus shown in FIG. 2, 200mL of a solvent, 4mL of acrylonitrile, 0.2mL of a 55% by mass dispersant solution, 0.1mL of 98% by mass concentrated sulfuric acid, 8mL of 2% by mass potassium persulfate solution, and 1mL of 10% by mass sodium thiosulfate solution were sequentially added to a 500mL three-necked flask.
And starting stirring after the feeding is finished, setting the stirring speed to be 200r/min, then starting the low-temperature water bath, setting the temperature of the low-temperature water bath to be 0 ℃, providing frozen saline water for the condenser pipe, finally starting the constant-temperature water bath, setting the temperature of the constant-temperature water bath to be 90 ℃, and continuing to react for 8 hours after the actual temperature of the constant-temperature water bath reaches a set value.
After the reaction is finished, the particle size of the product in the three-neck flask is measured by using a laser particle sizer, and the particle size is measured to be between 14 and 34 mu m.
Example 2
The detection apparatus shown in fig. 2 is used to carry out a specific detection process, and the detection apparatus shown in fig. 2 includes a stand 10, a thermometer 20, a container 30, a motor 40, a speed controller 50, a condenser 60, a constant temperature water bath 70, a low temperature water bath 80, and a stirring rod 90, wherein the container is a three-necked flask, one opening is used for inserting the stirring rod 90, the other opening is used for inserting the thermometer 20, the thermometer is used for measuring the temperature of a mixture in the container, the other opening is used for inserting the condenser 60, the container 30 is placed in the constant temperature water bath 70, the condenser 60 is communicated with the low temperature water bath 80, the low temperature water bath 80 is used for supplying cold water to the condenser, and the condenser is a condenser tube in.
The specific detection process comprises the following steps:
in the experimental apparatus shown in FIG. 2, 250mL of a solvent, 8mL of acrylonitrile, 0.8mL of a 30% by mass dispersant solution, 0.3mL of 98% by mass concentrated sulfuric acid, 16mL of a 2% by mass potassium persulfate solution, and 4mL of a 10% by mass sodium thiosulfate solution were sequentially added to a 500mL three-necked flask. And starting stirring after the feeding is finished, setting the stirring speed to be 200 r/min-240 r/min, then starting the low-temperature water bath, setting the temperature of the low-temperature water bath to be 10 ℃, providing frozen saline water for the condenser pipe, finally starting the constant-temperature water bath, setting the temperature of the constant-temperature water bath to be 70 ℃, and continuing to react for 6 hours after the actual temperature of the constant-temperature water bath reaches a set value. After the reaction, the particle size of the reaction solution is 320 to 700 μm.
Example 3
The procedure of the above experiment of example 1 was followed, except that the amount of the dispersant solution added was adjusted to 0.4mL and that the reaction solution had a particle size of 7 to 20 μm after the completion of the reaction.
Example 4
The difference from example 1; the amount of potassium persulfate solution added was adjusted to 12mL, and after the reaction was completed, the particle size of the reaction solution was 120 to 180. mu.m.
Example 5
The difference from example 1; the addition amount of the sodium thiosulfate solution is adjusted to 2mL, and after the reaction is finished, the granularity of the reaction solution is 80-130 μm.
Example 6
The difference from example 1; 170mL of solvent, 3.5mL of acrylonitrile, 0.15mL of 10% by mass dispersant solution, 0.75mL of 98% by mass concentrated sulfuric acid, 25mL of 1% by mass potassium persulfate solution and 0.15mL of 20% by mass sodium thiosulfate solution were sequentially added to a 500mL three-neck flask. And starting stirring after the feeding is finished, setting the stirring speed to be 200 r/min-240 r/min, then starting the low-temperature water bath, setting the temperature of the low-temperature water bath to be 10 ℃, providing frozen saline water for the condenser pipe, finally starting the constant-temperature water bath, setting the temperature of the constant-temperature water bath to be 50 ℃, and continuing to react for 7 hours after the actual temperature of the constant-temperature water bath reaches a set value. After the reaction, the particle size of the reaction solution is 210 to 310. mu.m.
Example 7
The difference from example 1; 170mL of a solvent, 25mL of acrylonitrile, 0.25mL of a 10% by mass dispersant solution, 0.5mL of 98% by mass concentrated sulfuric acid, 1.65mL of a 4% by mass potassium persulfate solution and 5mL of a 2% by mass sodium thiosulfate solution were sequentially added to a 500mL three-neck flask. And starting stirring after the feeding is finished, setting the stirring speed to be 200 r/min-240 r/min, then starting the low-temperature water bath, setting the temperature of the low-temperature water bath to be 10 ℃, providing frozen saline water for the condenser pipe, finally starting the constant-temperature water bath, setting the temperature of the constant-temperature water bath to be 50 ℃, and continuing to react for 7 hours after the actual temperature of the constant-temperature water bath reaches a set value. After the reaction, the particle size of the reaction solution is 380 to 440 μm.
Example 8
The difference from example 1; the mass percent of the dispersant is 9%. After the reaction, the particle size of the reaction solution was 2180 μm to 2400 μm.
Example 9
The difference from example 1; the volume of the dispersant was 0.1mL, which is 0.02% of the volume of the container. After the reaction, the particle size of the reaction solution is 900 to 1320 μm.
Example 10
The difference from example 1; the volume of the polymer acrylonitrile was 35 mL. After the reaction is finished, the granularity of the reaction liquid is 1480-1700 mu m.
Example 11
The difference from example 1; the volume of the solvent was 100 mL. After the reaction is finished, the granularity of the reaction solution is 1080-1300 mu m.
Example 12
The difference from example 1; the volume of concentrated sulfuric acid was 0.05 mL. After the reaction, the particle size of the reaction solution was 0 μm. The acrylonitrile in the reaction solution was not polymerized, and the effect of the dispersant could not be judged.
Example 13
The difference from example 1; the volume of the potassium persulfate solution was 1.5 mL. After the reaction, the particle size of the reaction solution was 0 μm. The acrylonitrile in the reaction solution was not polymerized, and the effect of the dispersant could not be judged.
Example 14
The difference from example 1; the mass percent of the potassium persulfate solution is 0.9 percent. After the reaction, the particle size of the reaction solution was 0 μm. The acrylonitrile in the reaction solution was not polymerized, and the effect of the dispersant could not be judged.
Example 15
The difference from example 1; the mass percent of the sodium thiosulfate solution is 21 percent. After the reaction, the particle size of the reaction solution is 1040 to 1330. mu.m.
Example 16
The difference from example 1; the volume of the sodium thiosulfate solution is 0.125 mL. After the reaction, the particle size of the reaction solution was 0 μm. The acrylonitrile in the reaction solution was not polymerized, and the effect of the dispersant could not be judged.
From the above description of the embodiments, when the mass percentage of the dispersant is 10-55%, the volume of the dispersant solution is 0.03-0.5% of the volume of the container, and the volume of the polymer to be polymerized is 1/150-1/20% of the volume of the container; in the concentrated sulfuric acid, the mass percent of sulfuric acid is 95-99%; in the composite initiator, the performance of the dispersant can be judged well when the mass percent of the potassium persulfate solution is between 1 and 4 percent, the mass percent of the sodium thiosulfate is between 1 and 20 percent, the volume of the concentrated sulfuric acid is 0.02 to 0.15 percent of the volume of the container, the volume of the potassium persulfate solution is 0.33 to 5 percent of the volume of the container, and the volume of the sodium thiosulfate solution is 0.03 to 1 percent of the volume of the container. In example 12, example 13, example 14 and example 16, acrylonitrile was not polymerized for a predetermined time due to poor initiation performance of the initiator.
From the above description, it can be seen that the above-described embodiments of the present application achieve the following technical effects:
according to the detection method, the dispersing agent and the polymer to be polymerized are added into the container, and then the container is heated to enable the polymer to be polymerized to react, so that the real situation in the recovery tower is simulated.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (15)
1. A method for testing the performance of a dispersant, the method comprising:
step S1, adding a dispersant solution and a polymer to be polymerized into a container to obtain a mixture;
step S2, heating the container to heat the mixture to a preset temperature and keep the temperature for a preset time to obtain a product; and
and step S3, measuring the granularity of the product, and judging the performance of the dispersing agent according to the granularity.
2. The detection method according to claim 1, wherein the mass percent of the dispersant in the dispersant solution is 10-55%, preferably the volume of the dispersant solution is 0.03-0.5% of the volume of the container, and the volume of the polymer to be detected is 1/150-1/20% of the volume of the container.
3. The detection method according to claim 1, wherein in the step S1, an initiator is further added to the container, and the mixture further comprises the initiator, preferably, the volume of the initiator is 0.38-6.15% of the volume of the container.
4. The detection method according to claim 3, wherein the initiator is a composite initiator, preferably the polymer is acrylonitrile, and the composite initiator comprises concentrated sulfuric acid, a potassium persulfate solution and a sodium thiosulfate solution.
5. The detection method according to claim 4, wherein the mass percent of sulfuric acid in the concentrated sulfuric acid is between 95 and 99 percent; in the potassium persulfate solution, the mass percent of the potassium persulfate solution is between 1 and 4 percent; in the sodium thiosulfate solution, the mass percent of the sodium thiosulfate is between 1 and 20 percent.
6. The detection method according to claim 4, wherein the volume of the concentrated sulfuric acid is 0.02 to 0.15% of the volume of the container, the volume of the potassium persulfate solution is 0.33 to 5% of the volume of the container, and the volume of the sodium thiosulfate solution is 0.03 to 1% of the volume of the container.
7. The detection method according to claim 1 or 3, wherein in the step S1, a solvent is further added to the container, and the mixture further includes the solvent, preferably the volume of the solvent is 1/3-1/2 of the volume of the container.
8. The detection method according to claim 1, wherein after the step S1, the detection method further comprises:
the mixture was stirred.
9. The detection method according to claim 8, wherein the stirring rate is between 200r/min and 240 r/min.
10. The method of claim 9, wherein the mixture is agitated by an agitation device comprising a stir bar, a speed governor, and a motor.
11. The detection method according to claim 1 or 8, characterized in that the detection method further comprises:
condensing the polymer to be polymerized in the gaseous state in the container, so that the polymer to be polymerized in the gaseous state is converted into the polymer to be polymerized in the liquid state.
12. The detection method according to claim 11, wherein the polymer to be detected in a gaseous state is condensed by a condenser, preferably the condenser is a condensation tube.
13. The detection method according to claim 1, wherein the predetermined temperature is 50-90 ℃ and the predetermined time is 6-8 h.
14. The method for detecting according to claim 1, wherein in the step S2, the container is heated by a constant temperature water bath.
15. The detection method according to claim 14, wherein the container is a three-necked flask, and the three-necked flask is placed in the constant temperature water bath.
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Application publication date: 20200218 |